Changes in the Microstructures and Inhibitors of Grain-Oriented Silicon Steel Under Different Normalizing Processes
YANG Weiyang1, LI Xianhao2, ZHAO Pengfei1,2, YU Haibin2, ZHAO Songshan2, LUO Haiwen1()
1 School of Metallurgical and Ecological Engineering, University of Science and Technology Beijing, Beijing 100083, China 2 Shougang Zhixin Qian'an Electromagnetic Materials Co. Ltd., Qian'an 064404, China
Cite this article:
YANG Weiyang, LI Xianhao, ZHAO Pengfei, YU Haibin, ZHAO Songshan, LUO Haiwen. Changes in the Microstructures and Inhibitors of Grain-Oriented Silicon Steel Under Different Normalizing Processes. Acta Metall Sin, 2024, 60(5): 605-615.
Normalizing is an important process that is widely employed in the industrial production of highly permeable grain-oriented silicon steel (GOSS). This is because it yields a proper microstructure, which is subsequently subjected to cold rolling, primary recrystallization, and secondary recrystallization-annealing. As a result, the sharpness Goss texture can be developed and GOSS posseses excellent magnetic properties. In this study, the influence of normalizing process parameters, including the heating rate, solution temperature, second-stage isothermal holding temperature and period for transformation, and cooling rate, on the resultant microstructures and inhibitors in the normalized GOSS were systematically investigated. Two types of distinct regions exist in the hot-rolled GOSS before normalization: the lamellar carbon-riched region elongated along the rolling direction, which is mainly composed of pearlite, and large ferrite region between the former regions. These two regions are alternately distributed from the subsurface to the center of the steel sheet. During heating and the solution processes, austenitization occurs only in the lamellar carbon-riched regions accompanying carbide dissolution, while no transformation occurs in the ferrite regions. An increase in either the solution temperature to up to 1200oC or its period to up to 3 min leads to the formation of more austenite. And the widely adopted solution condition of 1120oC for 3 min cannot dissolve all the formed lamellar carbides in the hot-rolled GOSS, leading to the nonuniform carbon concentration of the formed austenite in different regions. Consequently, some austenite can be retained after most of them transformed into martensite during water quenching. Moreover, all the results on microstructural characterization, in situ dilation experiment, and thermodynamic calculation show that austenitization continues to occur at the second-stage phase transformation temperature (900~950oC), instead of the commonly believed γ→α phase transformation. Therfore, inhibitor precipitation cannot be promoted by this phase transition. Furthermore, the fine nanosized inhibitors can precipitate in the ferrite region because the inhibitor's solubility is greatly reduced with decreasing temperature and in the pearlite regions accompany with the austenitic-to-pearlite transformation during air cooling below 900oC. An increase in the heating rate and solution temperature cause additional inhibitors in the hot-rolled GOSS to dissolve during the solution stage and reprecipitate to a fine size during the subsequent cooling. After normalization, the main types of inhibitors are AlN, the composite precipitates of AlN and MnS, and TiN.
Fund: National Natural Science Foundation of China(51831002);National Natural Science Foundation of China(52233018);Fundamental Research Founds for the Central Universities(FRF-TP-18-002C2)
Corresponding Authors:
LUO Haiwen, professor, Tel: (010)62332911, E-mail: luohaiwen@ustb.edu.cn
Fig.1 Schematics of normalizing processes of high permeability grain-oriented silicon steel (a) with the heating rates of 2, 10, and 50oC/s to 1120oC, samples named H2, H10, and H50, respectively (b) with the different solution temperatures of 950, 1000, 1120, and 1200oC, samples named S950, S1000, S1120, and S1200, respectively (c) with the additional stage of phase trans-formation at 950oC for 180 s, 900oC for 30 and 180 s, followed by water quenching, samples named P950, P900-1, and P900-2, respec-tively; and 900oC for 180 s followed by air cooling, sample named P900-2A
Fig.2 OM (a, d) and SEM (b, c) images of hot-rolled (a-c) and H2 normalized (d) grain-oriented silicon steel bands (ND—normal direction, RD—rolling direction, P—pearlite)
Fig.3 SEM images of grain-oriented silicon steel after the different normalizing processes (a-g) and EBSD quality map overlapped with phase map of retained austenite (h, i) (M—martensite) (a, h) S950 (b) S1000 (c) S1120 (d) S1200 (e, i) P900-2 (f) P950 (g) P900-2A
Fig.4 Dilatometric changes of grain-oriented silicon steel measured during the different normalizing processes (a, b) recorded dilations of S950, S1120, and S1200 samples varying with temperature (a) and time (b) (c) recorded dilation of P950 sample varying with time (Inset shows the locally enlarged curve) (d) recorded dilation of P900-2 varying with time (Inset shows the locally enlarged curve)
Fig.5 TEM images (a-c), EDS (d-g), and size distributions (h) of inhibitors in hot-rolled grain-oriented silicon steel plate
Fig.6 TEM images of inhibitors formed in H2 (a), H10 (b), and H50 (c, d) samples; corresponding EDS (e-g), average size and number density (h) and size distribution (i)
Fig.7 TEM images of inhibitors formed in S950 (a), S1000 (b), S1120 (c), and S1200 (d) samples; corresponding average size and number density (e), and size distributions (f)
Fig.8 TEM images of inhibitors formed in P900-1 (a), P900-2 (b), P950 (c), and P900-2A (d) samples; corresponding average size and number density (e) and size distributions (f)
Fig.9 Fe-C phase diagram for grain-oriented silicon steel with 0.1%Mn-3.25%Si, calculated by Thermo-Calc software and TCFE9 database
1
Günther K, Abbruzzese G, Fortunati S, et al. Recent technology developments in the production of grain-oriented electrical steel[J]. Steel Res. Int., 2005, 76: 413
doi: 10.1002/srin.2005.76.issue-6
2
Xia Z S, Kang Y L, Wang Q L. Developments in the production of grain-oriented electrical steel[J]. J. Magn. Magn. Mater., 2008, 320: 3229
doi: 10.1016/j.jmmm.2008.07.003
3
Liu G T, Yang P, Mao W M. Effect of final annealing atmosphere on secondary recrystallization behavior in thin gauge medium temperature grain oriented silicon steel[J]. Acta Metall. Sin., 2016, 52: 25
doi: 10.11900/0412.1961.2015.00200
Honda K, Kaya S, Masuyama Y. On the magnetic properties of single crystals of iron[J]. Nature, 1926, 117: 753
doi: 10.1038/117753a0
5
Dorner D, Zaefferer S, Lahn L, et al. Overview of microstructure and microtexture development in grain-oriented silicon steel[J]. J. Magn. Magn. Mater., 2006, 304: 183
doi: 10.1016/j.jmmm.2006.02.116
6
Kubota T, Fujikura M, Ushigami Y. Recent progress and future trend on grain-oriented silicon steel[J]. J. Magn. Magn. Mater., 2000, 215-216: 69
doi: 10.1016/S0304-8853(00)00069-X
7
Yang F Y, He C X, Meng L, et al. The effect of annealing atmosphere on the evolution behavior of inhibitors in thin-gauge grain-oriented silicon steel[J]. Mater. Trans., 2017, 58: 1524
doi: 10.2320/matertrans.M2017114
8
Wang Y, Zhu C Y, Li G Q, et al. Effect of decarburisation and nitriding on the carbon content, precipitates, microstructure and texture of Nb-bearing grain-oriented silicon steel[J]. Mater. High Temp., 2020, 37: 155
doi: 10.1080/09603409.2020.1731257
9
Song H Y, Wang Y P, Esling C, et al. The role of grain colony on secondary recrystallization in grain-oriented electrical steel: New insights from an original tracking experiment[J]. Acta Mater., 2021, 206: 116611
doi: 10.1016/j.actamat.2020.116611
10
Liao C C, Hou C K. Effect of nitriding time on secondary recrystallization behaviors and magnetic properties of grain-oriented electrical steel[J]. J. Magn. Magn. Mater., 2010, 322: 434
doi: 10.1016/j.jmmm.2009.09.072
11
Giri S K, Kundu S, Prakash A, et al. Defining the role of hot band annealing in high-permeability grain-oriented (GO) electrical steel[J]. Metall. Mater. Trans., 2022, 53A: 1873
12
Chang S K. Texture change from primary to secondary recrystallization by hot-band normalizing in grain-oriented silicon steels[J]. Mater. Sci. Eng., 2007, A452-453: 93
13
Li H, Feng Y L, Qi X J, et al. Study on microstructure and precipitates at different normalizing in Fe-3.15%Si low temperature oriented silicon steel[J]. Acta Metall. Sin., 2013, 49: 562
doi: 10.3724/SP.J.1037.2012.00644
Liu Y L, Zhu C Y, Jia J, et al. Effect of normalizing annealing temperature on precipitates and texture of Nb-Cr-bearing decarburized grain-oriented silicon steels[J]. Metals, 2019, 9: 457
doi: 10.3390/met9040457
15
Ling C, Xiang L, Qiu S T, et al. Effects of normalizing annealing on grain-oriented silicon steel[J]. J. Iron Steel Res. Int., 2014, 21: 690
doi: 10.1016/S1006-706X(14)60107-2
16
He Z Z, Zhao Y, Luo H W. Electrical Steel[M]. Beijing: Metallurgical Industry Press, 2012: 409
何忠治, 赵 宇, 罗海文. 电工钢[M]. 北京: 冶金工业出版社, 2012: 409
17
Cheng Z Y, Liu J, Yang J X, et al. Effect of normalization on the microstructure and texture evolution during primary and secondary recrystallization of Hi-B electrical steel[J]. Indian J. Eng. Mater. Sci., 2016, 23: 165
18
Tsai M C, Hwang Y S. The quenching effects of hot band annealing on grain-oriented electrical steel[J]. J. Magn. Magn. Mater., 2010, 322: 2690
doi: 10.1016/j.jmmm.2010.04.009
19
Fu B, Wang H J, Yan J X, et al. Effects of temperature and alloying elements on γ phase fraction of grain-oriented silicon steel[J]. J. Iron Steel Res. Int., 2016, 23: 573
doi: 10.1016/S1006-706X(16)30090-5
20
Wriedt H A. Solubility product of aluminum nitride in 3 percent silicon iron[J]. Metall. Trans., 1980, 11A: 1731
21
Wang X L, Luo L, Li W Z. Origin of fine equiaxed grains in industrial low-temperature grain-oriented silicon steel normalized sheet and their influence on magnetic properties[J]. J. Magn. Magn. Mater., 2022, 552: 169210
doi: 10.1016/j.jmmm.2022.169210
22
Wang R P, Li S D, Fang Z M, et al. Microstructure and precipitate of low temperature hot rolled HGO silicon steel plate by normalizing[J]. Heat Treat. Met., 2009, 34(6): 9
Giri S K, Durgaprasad A, Thool K, et al. High-temperature flow behaviour of grain-oriented and non-grain-oriented electrical steel[J]. Mater. Sci. Technol., 2019, 35: 1095
doi: 10.1080/02670836.2019.1612594
24
Sakai T, Shiozaki M, Takashina K. A study on AlN in high permeability grain-oriented silicon steel[J]. J. Appl. Phys., 1979, 50: 2369
doi: 10.1063/1.327007
25
Wang H J, Fu B, Xiang L, et al. Nucleation mechanism of precipitate of AlN in ferrite phase of Hi-B steel[J]. J. Iron Steel Res., 2015, 27(10): 40
Meng Z B, Zhao Y, He Z Z. Precipitation characteristic of nitride in high-induction grain-oriented silicon steel during normalizing[J]. Spec. Steel, 1999, 20(1): 24